国产甲磺酸多拉司琼有关物质的测定及其稳定性的初步研究  

Study on related substances and stability of dolasetron mesylate produced in China

作　　者：杨秀丽[1] 王东凯[1] 宋扬[1] 黎玲[1] 赵鹏[1] 苏娟娟[2] 

机构地区：[1]沈阳药科大学,沈阳110016 [2]沈阳沃森药物研究所,沈阳110016

出　　处：《药物分析杂志》2008年第1期80-84,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立 HPLC 法测定国产甲磺酸多拉司琼的有关物质,并初步考察其稳定性。方法:Diamonsil C_8(4.6 mm×250mm,5μm)色谱性;线性梯度洗脱,流动相 A 为0.008 mol·L^(-1)磷酸氢二铵溶液(磷酸调 pH 至7.0)-乙腈(200:16),流动相B为0.008 mol·L^(-1)磷酸氢二铵溶液(磷酸调 pH 至7.0)-乙腈(60:160);流速为1.0 mL·min^(-1);检测波长为210 nm;柱温为25℃;进样量为100 μL。结果:建立了 HPLC 法,可同时测定甲磺酸多拉司琼中甲磺酸多拉司琼有关物质 A 和其他杂质的含量。有关物质 A 浓度在0.36～14.4μg·mL^(-1)范围内与峰面积呈良好的线性关系,回归方程为 Y=1.169×10^(-4)X-1.491×10~3,r=0.9993,最低检测限为120 ng,回收率(n=9)为100.0%。对甲磺酸多拉司琼的稳定性进行了初步考察,在光照条件下,有关物质稍有变化;高湿条件下,性状稍有变化;在其他影响因素试验、加速试验和长期试验中,甲磺酸多拉司琼的性状和有关物质均无明显变化,表明甲磺酸多拉司琼在贮藏过程中基本稳定。结论:该法方法简便、快速、准确,适合该药生产和制剂的质量控制。Objective： To establish an HPLC method for assay the related substances in domestic dolasetron mesylate and to study its stability. Method：A Diamonsil Cs （4.6 mm× 250 mm, 5 μm） column was used for the gradient elution. The mobile phase A was 0. 008 mol · L^- 1 dibasic ammonium phosphate solution （ adjust to pH 7.0 with phosphoric acid） - acetonitrile（200： 16） ;The mobile phase B was 0. 008 mol · L^-1 dibasic ammonium phosphate solution（ adjust to pH 7.0 with phosphoric acid） -acetonitrile（60： 160）. The flow rate was 1.0 mL·min^-1, the detective wavelength was 210 nm, the column temperature was 25 ℃, the injection volume was 100 μL. Results：Dolasetron mesylate related compound A and other related substances were detected by the established method. The calibration curve was linear in the concentration range of 0. 36 - 14. 4 μg · mL^- 1 （ r = 0. 9993） for dolasetron mesylate related compound A and the regression equation being Y = 1. 169 × 10^4X - 1. 491 × 10^3, and the detection limit was 120 ng ;The recovery（ n = 9） of assay was 100.0%. The stability of dolasetron mesylate was studied. It can be concluded that：under light conditions, the content of related substances was slightly changed;under high humidity conditions its appearance was slightly changed;in other tests including accelerated test and long - term test, its appearance and content were not obviously changed. Conclusion ：This method is simple, convenient, fast, accurate, and can be applied for manufacture and quality control of the preparation.

关 键 词：甲磺酸多拉司琼 有关物质 HPLC法 稳定性 

分 类 号：R917[医药卫生—药物分析学]